CN105878335A - Quality control and preparation method of Chinese herbal medicine particles with single component - Google Patents
Quality control and preparation method of Chinese herbal medicine particles with single component Download PDFInfo
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Abstract
The invention relates to quality control and a preparation method of Chinese herbal medicine particles with a single component. The method mainly comprises the following steps: 6300g of Lespedeza cuneata is taken, water is added for carrying out twice decoction, a first decoction is carried out for 2 hours, a second decoction is carried out for 1.5 hours, filtration is carried out, filtrates are merged, and condensation is carried out in order to obtain a thick paste whose relative density is about 1.30 (60 DEG C); ethyl alcohol is added in order to ensure the alcohol content of the thick paste which reaches to 60%, the thick paste is allowed to stand, filtration is carried out, filtrate is taken for recycling ethyl alcohol, condensation is carried out in order to obtain a dry paste, and the dry paste is pulverized and sieved; talcum powder is added till the total weight is 950g, well mixing is carried out, pills are processed with water, 50g of a mixture containing talcum powder and ferric oxide is used for coating, wherein the weight of talcum powder and the weight of ferric oxide are identical, drying is carried out, polishing is carried out, and 1000g of the particles are prepared. The particles have the beneficial effects of astringency, antidiarrheal effect, simple preparation, low cost, stable drug effects, etc.; the particles are helpful for treating diarrhea, dyspepsia, acute gastroenteritis, and other illnesses.
Description
Technical field
The present invention relates to the compound method of a kind of drug particles, particularly relate to quality control and the compound method of a kind of single Chinese herb medicine particle.
Background technology
Cuneate lespedeza is pulse family Lespedeza plant lespedeza cuneata Lespedeza cuneata (Dum-Cours.) G.Don, and stem is cylinder, and stem, branch matter are the most crisp, frangibility, and section has marrow；Gas is micro-, and taste is sweet, micro-hardship；Top branch, surface red brown or kermesinus, tool substantially thin longitudinal grin or shallow ridges, spray epimere is pasted hair by white, the few hair of old branch；Leaf comes off more, residual petiolule or leaf scar；Leaf three goes out answers alternate, and two consor of minority are intensive；On petiole three leaflets, strip wedge shape, tip is truncate, and there are stimuli in central authorities；This medicine clearing heat and promoting diuresis, help digestion except long-pending, expelling phlegm and arresting coughing, can be used for infantile malnutrition, indigestion, gastroenteritis, bacillary dysentery, stomachache, icteric hepatitis, nephritic dropsy, stomatitis, cough, bronchitis etc..At present for Chinese medicine preparation, lack the drug particles contributing to alleviating and cure the aspects such as diarrhoea, indigestion, acute gastroenteritis, simultaneously, the preparation quality of other similar drugs also exists again certain difference, and these factors all can cause seeming the most effective when tackling " astringing to arrest diarrhea " this symptom.
This case relates to Chinese herb medicine " cuneate lespedeza ", and its active component is the material base of its curative effect, and foundation gram is rushed down quick granular mass and controlled standard, meets the modern Chinese herbal medicine quality of the pharmaceutical preparations and controls system, is to ensure human administration's safely and effectively important evidence.Accordingly, it would be desirable to combine this medicine of cuneate lespedeza to carry out the innovation of compound method.
Summary of the invention
For disadvantages described above, the present invention provides a kind of astringing to arrest diarrhea, preparation is easy, cost is relatively low, the quality control of the single Chinese herb medicine particle of efficacy stability and compound method, thus for indigestion, acute gastroenteritis etc..
For achieving the above object, the present invention is by the following technical solutions:
The quality control of a kind of single Chinese herb medicine particle and compound method, mainly comprise the steps that
(1) take cuneate lespedeza 6300g, boiling secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, be condensed into relative density and be about the thick paste of 1.30 (60 DEG C)；
(2) adding ethanol makes the alcohol content of above-mentioned thick paste reach 60%, stands, filters, take filtrate recycling ethanol, and the dry cream being condensed into is pulverized, sieved；
(3) adding talcum powder to total amount is 950g, mixing, and with water pill, by the mixture 50g coating altogether of talcum powder with di-iron trioxide, talcum powder therein is equal in weight with di-iron trioxide, is dried, polishing, makes 1000g.
Identification method: use thin-layered chromatography to identify, comprise the following steps:
(1) need testing solution preparation takes this product 1.5g, finely ground, adds ethanol 25ml, ultrasonically treated (power 240W, frequency 33kHz) 30 minutes, filters, filtrate water bath method, residue adds hot water 15ml makes dissolving, filters, the n-butanol shaking that filtrate water is saturated is extracted 2 times, and each 15ml merges n-butanol, the water 15ml saturated with n-butanol washs 1 time, divides and takes n-butanol liquid, water bath method, residue adds ethanol 2ml makes dissolving, to obtain final product；
(2) preparation of control medicinal material solution takes cuneate lespedeza control medicinal material 2g, finely ground, add diethyl ether 30ml, ultrasonically treated (power 240W, frequency 33kHz) 20 minutes, discard ether solution, residue volatilizes, add ethanol 25ml, ultrasonically treated (power 240W, frequency 33kHz) 30 minutes, filter, filtrate water bath method, residue adds hot water 15ml makes dissolving, filter, the n-butanol shaking that filtrate water is saturated is extracted 2 times, 15ml every time, merge n-butanol extracting liquid, add the saturated water 15ml of n-butanol again to wash 1 time, divide and take n-butanol liquid, water bath method, residue adds ethanol 2ml makes dissolving, obtain；
(3) above-mentioned test sample, each 1 μ l of control medicinal material solution are drawn, respectively to put on same polyam ide TLC plate, with n-butanol-ethanol-glacial acetic acid (8: 4: 1) as solvent, launch, taking out, dry, spray is with 3% alchlor ethanol solution, volatilize or hot blast drying, put and inspect under ultraviolet lamp (365nm).In test sample chromatogram, on position corresponding with control medicinal material chromatogram, aobvious identical fluorescence spot.
Assay: include following condition and step.
Chromatographic condition and system suitability test are with octadecylsilane chemically bonded silica as filler, and with acetonitrile as mobile phase A, 0.5 glacial acetic acid solution is Mobile phase B, and the regulation according to the form below carries out gradient elution；Detection wavelength is 256nm.Number of theoretical plate is calculated by quercitin peak should be not less than 4000.
(1) preparation of reference substance solution: accurately weighed quercitin reference substance 0.01g, puts in 20ml measuring bottle, adds methyl alcohol and be dissolved to scale, precision measures 2.5ml, is placed in 50ml measuring bottle, adds methanol constant volume to scale, shake up, obtain reference substance solution (about 25 μ g/ml)；
(2) preparation of need testing solution: take same batch sample, finely ground, take 2.5g, accurately weighed, put in 50ml conical flask, add methyl alcohol 25ml, weighed weight, ultrasonically treated (300W, 45kHz) 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with methyl alcohol, shaking up, filter, precision measures subsequent filtrate 10ml, after flinging to part methyl alcohol, quantitatively transfer is put in 5ml measuring bottle, with methanol dilution to scale, shakes up, filter, take subsequent filtrate, to obtain final product；
(3) measure: precision draws reference substance solution 10 μ l respectively, inject liquid chromatograph, measure, to obtain final product；
Regulation this product every bag contains cuneate lespedeza with quercitin (C21H20O11) must not count less than 1.0mg.
Described drug particles applies also for tablet, pill, capsule.
Additionally, above-mentioned for gram rushing down quick particle, relevant every regulation under granule item should be met.(Chinese Pharmacopoeia one annex IL of version in 2010).
The particle every bag 15g prepared, seals storage.Be that boiling water is taken after mixing it with water during use, one time 1～2 bag, 3 times on the one.
Quality control and the having the beneficial effect that of compound method of single Chinese herb medicine particle of the present invention have the advantage such as astringing to arrest diarrhea, preparation simplicity, relatively low, the efficacy stability of cost；Contribute to treating the illnesss such as astringing to arrest diarrhea, diarrhoea, indigestion, acute gastroenteritis.
Detailed description of the invention
The quality control of the single Chinese herb medicine particle described in the embodiment of the present invention and compound method, as a example by 1000g, mainly comprise the steps that
(1) take cuneate lespedeza 6300g, boiling secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, be condensed into relative density and be about the thick paste of 1.30 (60 DEG C)；
(2) adding ethanol makes the alcohol content of above-mentioned thick paste reach 60%, stands, filters, take filtrate recycling ethanol, and the dry cream being condensed into is pulverized, sieved；
(3) adding talcum powder to total amount is 950g, mixing, and with water pill, by the mixture 50g coating altogether of talcum powder with di-iron trioxide, talcum powder therein is equal in weight with di-iron trioxide, is dried, polishing, makes 1000g.
Thering is provided its operability for those skilled in the art, analysis below is merely to illustrate the present invention, and it limits the scope of the present invention never in any form, and following experimental technique is conventional method, and raw and auxiliary material used is the raw and auxiliary material product of national regulation.
(1) thin-layer chromatography is identified
Reagent and reagent
1. sample: gram rush down quick particle, totally 8 batches, lot number is respectively 090801,090802,090803,100301,100302,100401,100402,100501, is provided by Guangdong Yongkang Pharmaceutical Co., Ltd..
2. the preparation of need testing solution: take this product 1.5g, finely ground, add ethanol 25ml, ultrasonically treated (power 240W, frequency 33kHz) 30 minutes, filters, filtrate water bath method, residue adds hot water 15ml makes dissolving, filters, the n-butanol shaking that filtrate water is saturated is extracted 2 times, and each 15ml merges n-butanol, the water 15ml saturated with n-butanol washs 1 time, divides and takes n-butanol liquid, water bath method, residue adds ethanol 2ml makes dissolving, as need testing solution.
3. the preparation of control medicinal material solution: take cuneate lespedeza control medicinal material 2g, finely ground, add diethyl ether 30ml, ultrasonically treated (power 240W, frequency 33kHz) 20 minutes, discard ether solution, residue volatilizes, add ethanol 25ml, ultrasonically treated (power 240W, frequency 33kHz) 30 minutes, filter, filtrate water bath method, residue adds hot water 15ml makes dissolving, filter, the n-butanol shaking that filtrate water is saturated is extracted 2 times, 15ml every time, merge n-butanol extracting liquid, add the saturated water 15ml of n-butanol again to wash 1 time, divide and take n-butanol liquid, water bath method, residue adds ethanol 2ml makes dissolving, make control medicinal material solution.
4. the preparation of negative control solution: take the amount being equivalent to test sample, makes negative control solution by the preparation method of need testing solution.
5. lamellae: polyam ide TLC plate.
6. experimental situation: temperature 28 DEG C, relative humidity 65%
7. point sample, launch, inspect: draw each 1 μ l of above-mentioned test sample, control medicinal material solution and negative control solution, respectively with point-like point on same polyam ide TLC plate, with n-butanol-ethanol-glacial acetic acid (8: 4: 1) as solvent, launch, taking out, dry, spray is with 3% alchlor ethanol solution, volatilize or hot blast drying, put and inspect under ultraviolet lamp (365nm).
In chromatogram, on position corresponding with cuneate lespedeza control medicinal material, aobvious identical fluorescence spot, negative noiseless.
8. the selection of method:
(1) lamellae: compare silica G plate and polyam ide TLC plate, finds the latter's good separating effect.(2) solvent: following two kinds of solvents
Ethyl acetate-alcohol-water-glacial acetic acid (8: 2: 1: 1)
N-butanol-ethanol-glacial acetic acid (8: 4: 1)
Result: n-butanol-ethanol-glacial acetic acid (8: 4: 1) is that the effect of solvent is good.
(3) point sample amount is investigated
Gram rushing down quick particle is prepared by need testing solution preparation method, respectively point sample 2 μ l and 1 μ l.Result shows that 2 μ l point sample amounts are excessive, and spot hangover is serious, and separating degree is the best, therefore selecting point sample amount is 1 μ l.
(4) comparison of difference sample loading mode
Respectively with point-like and banding point plate, comparing both effects, result shows two kinds of point sample modes.
9. Method validation
(1) specificity this product fixs one's mind on taste Chinese herbal and crude drugs preparations, and negative control is noiseless
(2) investigation of durability
1) comparison of the polyam ide TLC plate of different lot numbers: result display no significant difference.
2) comparison of different temperatures: take the lamellae after point sample, launch at 8 DEG C with 28 DEG C respectively, colour developing, to inspect under ultraviolet light (365nm), result shows: test at 8 DEG C with 28 DEG C, on differentiating without significantly impact.
3) comparison of different humidity: investigate under low humidity (32%) and high humidity (72%) expansion effect respectively, result shows under relative humidity 32% and 72% time test, on differentiating without significantly impact.
(2) content assaying method
HPLC method mensuration gram is used to rush down the content of quercitin in quick particle.
1. test material
(1) instrument: Waters high performance liquid chromatograph, chromatographic column: Hibar C18 (5 μm .250 × 4.6mm).Balance: PrecisaXT200A electronic balance, SartoriusCP224S electronic balance, SartoriusCP225D electronic balance.VOS-201SD vacuum drying chamber.
(2) reagent: HPLC second is fine for chromatographically pure: HPLC water is ultra-pure water；Other reagent is pure for analyzing.
(3) test specimen gram rushes down quick particle (lot number: 090801,090802,090803,100301,100302,100401,100402,100501 is provided) by Guangdong Yongkang Pharmaceutical Co., Ltd.；Gram rush down quick particle negative control (Guangdong Yongkang Pharmaceutical Co., Ltd.'s offer)；Quercitin (lot number 11538-200403, Nat'l Pharmaceutical & Biological Products Control Institute).
2. Method validation
(1) accuracy test (sample-adding reclaims)
The preparation of reference substance solution: accurately weighed quercitin reference substance 0.00988g, puts in 20ml measuring bottle, adds methyl alcohol and be dissolved to scale, obtain stock solution；Precision measures stock solution 2ml and puts in 200ml, adds methanol dilution to scale, as reference substance solution (that is: 4.94 μ g/ml).
Sample-adding reclaims the preparation of solution: take known content gram rushes down quick particle (lot number 100402 Determination of Quercitrin is 0.1008mg/g) 6 parts, and every part takes 1.25g, accurately weighed, puts in 50ml conical flask, accurate adds quercitin reference substance solution 25ml.Prepare by need testing solution preparation method, measure.The rate of recovery is shown in Table 1.Knowable to following table, average recovery rate is 103.7, and RSD is 1.0%, illustrates that the degree of accuracy of this method is high.
Table 1 is loaded recovery test result
(2) precision test
1) replica test
The preparation of reference substance solution: the accurate stock solution 2.5ml drawn under accuracy test item, is placed in 50ml measuring bottle, adds methanol constant volume to scale, shakes up, obtain reference substance solution (i.e. 24.7 μ g/ml).
The preparation of need testing solution: take same batch sample (lot number 100402), mixing, take 6 parts, every part of 2.5g, accurately weighed, put in 50ml conical flask, add methyl alcohol 25ml, weighed weight, ultrasonically treated (300W, 45kHz) 30 minutes, lets cool, more weighed weight, supplying the weight of less loss with methyl alcohol, shake up, filter, precision measures subsequent filtrate 10ml, after flinging to part methyl alcohol, quantitatively transfer is put in 5ml measuring bottle, with methanol dilution to scale, shakes up, filter, take subsequent filtrate, to obtain final product.Measurement result is shown in Table 2.
Table 2 replica test result
As shown in Table 2: this law repeatability is good.
2) Intermediate precision test
Taking two batch samples (100401,100501) respectively, 2 bit test persons prepare need testing solution the most in accordance with the law, operate according to method under assay item, measure the content of quercitin, the results are shown in Table 3.
Table 3 quercitin Intermediate precision result of the test (n=8)
Table 3 result shows, the method Intermediate precision is good.
3. specificity
The preparation of reference substance solution: same to replica test.
The preparation of need testing solution: same to replica test.
Prepared by negative control solution: take negative sample 2.5g, makes negative control solution with need testing solution preparation method.
Draw each 10 μ l of reference substance solution, need testing solution and negative control solution respectively, inject liquid chromatograph, measure by content assaying method.
Result: quercitin reference substance retention time is 44.026 minutes, peak area is 663579, and in test sample (lot number 100302), quercitin retention time is 44.055 minutes, peak area is 582732, negative sample at corresponding retention time without chromatographic peak, noiseless, meet the requirements.
4. linear relationship
The accurate stock solution 3ml drawn under accuracy test item, is placed in 100ml measuring bottle, adds methanol constant volume to scale, shakes up, obtain reference substance solution (i.e. 14.82 μ g/ml).
Taking above-mentioned reference substance solution 2,6,10,15,25 μ l respectively, inject in liquid chromatograph, gained linear relationship data (is shown in Table 4).With reference substance concentration (ng) as abscissa (X), peak area is ordinate (Y)
Drawing to obtain straight line, regression equation is as follows: y=2499.0x+13934.4, R=1.0000, illustrate quercitin in the range of 29.64ng～370.5ng in good linear relationship.It is shown in Table 4 linear regression result of the tests.
Table 4 linear regression result of the test
5. durability is investigated
(1) selection of different extraction times
Taking this product 4 parts, every part of about 2.5g, difference is the most accurately weighed, puts in 50ml conical flask, add methyl alcohol 25ml, weighed weight, respectively ultrasonically treated (300W, 45kHz) 20,30,45,60 minutes, let cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filtering, precision measures subsequent filtrate 10ml, after flinging to part methyl alcohol, quantitatively transfer is put in 5ml measuring bottle, with methanol dilution to scale, shakes up, filter, take subsequent filtrate, to obtain final product.
The results are shown in Table 5.
Table 5 different extraction time investigates result
As shown in Table 5, the extraction effect of 4 kinds of different ultrasonic times is suitable, the preparation method of need testing solution with ultrasonic time 30 minutes as extracting method.
(2) the different selections extracting liquor capacity
Take this product every part about 2.5g, the most accurately weighed, put in 50ml conical flask, respectively precision add methyl alcohol 15,25,50ml, weighed weight, ultrasonically treated (300W, 45kHz) 30 minutes, let cool respectively, the most weighed weight, supplies the weight of less loss, shakes up with methyl alcohol, filtering, precision measures subsequent filtrate 10ml, after flinging to part methyl alcohol, quantitatively transfer is put in 5ml measuring bottle, with methanol dilution to scale, shakes up, filter, take subsequent filtrate, to obtain final product.The results are shown in Table 6.
Table 6 different solvents volume investigates result
(3) selection of wavelength is measured
Taking the flowing phase solution of quercitin reference substance, with flowing for blank, scan in the range of 200-400nm, result has absorption maximum at 256nm wavelength, so determining that detection wavelength is 256nm.
(4) selection of the phase that flows
Quercitin slightly trails in HPLC separates.For improving peak shape, bibliography, investigate methyl alcohol-0.2% glacial acetic acid solution, acetonitrile-0.2% glacial acetic acid solution, acetonitrile-0.5% glacial acetic acid solution respectively, finally select acetonitrile-0.5% glacial acetic acid solution as flowing phase.Having investigated isocratic and gradient elution, because chromatographic peak is more in sample, the final quercitin used in gradient elution mode separation sample, separating degree is good.
(5) study on the stability
Taking with a need testing solution (lot number: 100302), respectively at 0,4,8,12,18,24 hours, inject high performance liquid chromatograph, note down peak area, result shows that detected solution is stable in 24 hours, is shown in Table 7.
Table 7 stability test result
(6) study on the stability
Take with a need testing solution (lot number: 100402), operate according to method under assay item, use the chromatographic column mensuration gram of 3 different sizes to rush down the content of quercitin in quick particle, the results are shown in Table 8.
Chromatographic column: (1) Hibar C18 (5 μm, 4.6mm × 250mm)
(2) Phenomenex (5 μm, 4.6mm × 250mm)
(3) SHISEIDO (5 μm, 4.6mm × 250mm)
The different chromatographic column of table 8 investigates result
(3) method using embodiment 2 to determine, takes 8 batch samples collected, and measures according to the method drafted, the results are shown in Table 9.
Table 9 assay result
(4) assay of medicinal material
Taking production cuneate lespedeza medicinal material used to keep sample (lot number: 090701), 090801 grade eight batches grams provided for producer rushes down the preparation of quick particle, measures Determination of Quercitrin in accordance with the law, calculates the rate of transform of Determination of Quercitrin, the results are shown in Table 10.
The rate of transform of Determination of Quercitrin in table 10 medicinal material
(5) determination of limit
Due to control without quercitin in cuneate lespedeza quality standard, therefore the limit of finished product cannot be calculated according to the rate of transform.According to the 8 ratio sample result surveyed, its average content is 1.5mg/ bag, it is contemplated that industrialization and the impact of crude drug source factor, intends being set to limit with the 70% of average, and i.e. every bag contains cuneate lespedeza with quercitin (C21H20O11) meter, 1.0mg must not be less than.
In pill, the quercitin rate of transform is only in granule about the 50% of the quercitin rate of transform, thus the former quercitin limit value press that the conversion of cuneate lespedeza inventory is the latter 50%.This is likely due to, and the preparation method of two kinds of formulations is inconsistent to be caused.Above-mentioned method of quality control is applicable not only to granule, is simultaneously suitable for pill.Raw material dose contained by raw material dose used by pill and above-mentioned granule is identical.
Specific description of embodiments of the present invention above is not limiting as the present invention, and those skilled in the art can be variously modified according to the present invention or deform, and without departing from the spirit of the present invention, all should belong to scope of the following claims of the present invention.
Claims (4)
1. the quality control of a single Chinese herb medicine particle and compound method, it is characterised in that mainly comprise the steps of:
(1) take cuneate lespedeza 6300g, boiling secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, be condensed into relative density and be about the thick paste of 1.30 (60 DEG C)；
(2) adding ethanol makes the alcohol content of above-mentioned thick paste reach 60%, stands, filters, take filtrate recycling ethanol, and the dry cream being condensed into is pulverized, sieved；
(3) adding talcum powder to total amount is 950g, mixing, and with water pill, by the mixture 50g coating altogether of talcum powder with di-iron trioxide, talcum powder therein is equal in weight with di-iron trioxide, is dried, polishing, makes 1000g.
The quality control of single Chinese herb medicine particle the most according to claim 1 and compound method, it is characterised in that drug particles uses thin-layered chromatography to identify, comprises the following steps:
(1) prepared by need testing solution: take this product 1.5g, finely ground, adds ethanol 25ml, ultrasonically treated 30 minutes, filter, filtrate water bath method, residue adds hot water 15ml makes dissolving, filters, and the n-butanol shaking that filtrate water is saturated is extracted 2 times, 15ml every time, merges n-butanol, and the water 15ml saturated with n-butanol washs 1 time, divide and take n-butanol liquid, water bath method, residue adds ethanol 2ml makes dissolving, to obtain final product；
(2) preparation of control medicinal material solution takes cuneate lespedeza control medicinal material 2g, finely ground, add diethyl ether 30ml, ultrasonically treated 20 minutes, discard ether solution, residue volatilizes, and adds ethanol 25ml, ultrasonically treated 30 minutes, filter, filtrate water bath method, residue adds hot water 15ml makes dissolving, filters, the n-butanol shaking that filtrate water is saturated is extracted 2 times, 15ml every time, merges n-butanol extracting liquid, then adds the saturated water 15ml washing of n-butanol 1 time, divide and take n-butanol liquid, water bath method, residue adds ethanol 2ml makes dissolving, to obtain final product；
(3) above-mentioned test sample, each 1 μ l of control medicinal material solution are drawn, respectively to put on same polyam ide TLC plate, with n-butanol-ethanol-glacial acetic acid as solvent, launch, take out, dry, spray, with 3% alchlor ethanol solution, volatilizes or hot blast drying, puts and inspect under ultraviolet lamp.In test sample chromatogram, on position corresponding with control medicinal material chromatogram, aobvious identical fluorescence spot.
The quality control of single Chinese herb medicine particle the most according to claim 1 and compound method, it is characterised in that the mensuration of drug particles content, including following condition and step:
(1) preparation of reference substance solution: accurately weighed quercitin reference substance 0.01g, puts in 20ml measuring bottle, adds methyl alcohol and be dissolved to scale, and precision measures 2.5ml, is placed in 50ml measuring bottle, adds methanol constant volume to scale, shakes up, obtain reference substance solution；
(2) preparation of need testing solution: take same batch sample, finely ground, take 2.5g, accurately weighed, put in 50ml conical flask, add methyl alcohol 25ml, weighed weight, ultrasonically treated 30 minutes, let cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filtering, precision measures subsequent filtrate 10ml, after flinging to part methyl alcohol, quantitatively transfer is put in 5ml measuring bottle, with methanol dilution to scale, shakes up, filter, take subsequent filtrate, to obtain final product；
(3) measure: precision draws reference substance solution 10 μ l respectively, inject liquid chromatograph, measure, to obtain final product.
The quality control of single Chinese herb medicine particle the most according to claim 1 and compound method, it is characterised in that described drug particles applies also for tablet, pill, capsule.
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| CN107132307A (en) * | 2017-05-08 | 2017-09-05 | 山东省中医药研究院 | A kind of cacumen biotae TLC discrimination methods |
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Application publication date: 20160824 |